WO2019240063A1 - 積層部材の製造方法 - Google Patents

積層部材の製造方法 Download PDF

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Publication number
WO2019240063A1
WO2019240063A1 PCT/JP2019/022882 JP2019022882W WO2019240063A1 WO 2019240063 A1 WO2019240063 A1 WO 2019240063A1 JP 2019022882 W JP2019022882 W JP 2019022882W WO 2019240063 A1 WO2019240063 A1 WO 2019240063A1
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WIPO (PCT)
Prior art keywords
flame
adhesive
treatment
resin
dry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2019/022882
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English (en)
French (fr)
Inventor
愛美 阿部
裕一 松木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yokohama Rubber Co Ltd
Original Assignee
Yokohama Rubber Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yokohama Rubber Co Ltd filed Critical Yokohama Rubber Co Ltd
Priority to CN201980033630.XA priority Critical patent/CN112154066B/zh
Priority to US16/973,969 priority patent/US11254114B2/en
Priority to EP19818538.1A priority patent/EP3808559A4/en
Publication of WO2019240063A1 publication Critical patent/WO2019240063A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0036—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
    • B29C66/028—Non-mechanical surface pre-treatments, i.e. by flame treatment, electric discharge treatment, plasma treatment, wave energy or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/4805—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the type of adhesives
    • B29C65/483—Reactive adhesives, e.g. chemically curing adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/4805—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the type of adhesives
    • B29C65/483—Reactive adhesives, e.g. chemically curing adhesives
    • B29C65/485—Multi-component adhesives, i.e. chemically curing as a result of the mixing of said multi-components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
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    • B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
    • B29C66/45—Joining of substantially the whole surface of the articles
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    • B29C66/737—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined
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    • B29C66/737—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined
    • B29C66/7377—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline
    • B29C66/73775—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline the to-be-joined area of at least one of the parts to be joined being crystalline
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7392—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/746—Joining plastics material to non-plastics material to inorganic materials not provided for in groups B29C66/742 - B29C66/744
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
    • B29C65/521—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive by spin coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
    • B29C65/522—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive by spraying, e.g. by flame spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
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    • B29C65/524—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive by applying the adhesive from an outlet device in contact with, or almost in contact with, the surface of the part to be joined
    • B29C65/525—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive by applying the adhesive from an outlet device in contact with, or almost in contact with, the surface of the part to be joined by extrusion coating
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Definitions

  • the present invention relates to a method for manufacturing a laminated member.
  • a manufacturing method of a laminated member for producing a laminated member having this order a surface treatment step of performing a dry treatment so as to satisfy a specific condition on the surface of the first member containing a crystalline thermoplastic resin;
  • an adhesive is applied to the surface of the first member subjected to the dry treatment without using a primer composition, and an adhesive layer is formed on the surface of the first member subjected to the dry treatment.
  • a method for manufacturing a laminated member has been proposed that includes an adhesive application step and a bonding step in which a second member is bonded onto the adhesive layer (for example, Patent Document 1).
  • an object of the present invention is to provide a method for producing a laminated member that exhibits excellent adhesion without using a primer.
  • the present inventors have found that the above problems can be solved by performing a dry treatment so as to satisfy a specific condition for a member containing a crystalline thermoplastic resin. That is, the present inventors have found that the above problem can be solved by the following configuration.
  • a method for producing a laminated member comprising producing a laminated member having a first member containing a crystalline thermoplastic resin, an adhesive layer, and a second member in this order, A surface treatment step of performing a dry treatment on the surface of the first member containing the crystalline thermoplastic resin so as to satisfy the following condition A; Adhesive is applied to the surface of the first member subjected to the dry treatment without using a primer composition, and an adhesive layer is formed on the surface of the first member subjected to the dry treatment.
  • Agent application step The manufacturing method of a laminated member provided with the bonding process of bonding a 2nd member on the said adhesive bond layer.
  • the dry treatment of the first member is a flame treatment, and a flame of reducing flame is applied to the surface of the first member in the flame treatment.
  • the adhesive is at least one selected from the group consisting of urethane adhesives, epoxy adhesives, modified silicone adhesives, and acrylic adhesives.
  • the manufacturing method of the laminated member in any one of.
  • the second member contains a crystalline thermoplastic resin
  • a surface treatment step for performing a dry treatment on the surface of the second member so as to satisfy the following condition A2,
  • the dry treatment of the second member is a flame treatment, and a flame of reducing flame is applied to the surface of the second member in the flame treatment.
  • FIG. 1 is a schematic cross-sectional view showing an embodiment of the production method of the present invention in the order of steps.
  • a numerical range represented by using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
  • the method for producing a laminated member of the present invention includes a first member containing a crystalline thermoplastic resin, an adhesive layer, and a second member in this order. Is a method for manufacturing a laminated member, comprising the following three steps.
  • Process 1 Surface treatment process The process of performing a dry process so that the conditions A mentioned later may be satisfy
  • Process 2 Adhesive provision process Above A step of forming an adhesive layer on the surface of the first member subjected to the dry treatment by applying an adhesive to the surface of the first member subjected to the dry treatment without using a primer composition (3 )
  • Step 3 bonding step The step of bonding the second member on the adhesive layer.
  • the method of this invention takes such a structure, it is estimated that the obtained laminated body shows the outstanding adhesiveness. The reason is not clear, but it is presumed that it is as follows.
  • the surface of the member containing the crystalline thermoplastic resin is dry-treated so as to satisfy the condition A described below (hereinafter, the condition A is also referred to as “specific condition”).
  • the condition is milder than the case where the flame is exposed to an oxidization flame (outer flame), and it is possible to suppress excessive treatment by dry treatment, and the surface of the member is hydrophilic without breaking the crystallinity of the outermost surface of the member.
  • an adhesive layer is formed on the surface of the hydrophilicized member so that the adhesive layer is sufficiently adhered to the entire surface, and the adhesive layer formed from the adhesive layer has a crystal structure on the outermost surface of the member. It is considered that it becomes an anchor and is firmly fixed to the member. As a result, it is considered that a laminated member exhibiting excellent adhesiveness can be obtained without using a primer composition.
  • FIG. 1 is a schematic cross-sectional view showing an embodiment of the production method of the present invention in the order of steps.
  • FIG. 1A shows the first member 10 used in the surface treatment process.
  • a dry treatment is performed on the surface 10a of the first member 10 so as to satisfy a specific condition.
  • the 1st member 12 after a dry process is obtained (FIG.1 (b)).
  • the adhesive application step the adhesive is applied to the surface 12a subjected to the dry treatment of the first member 12 after the dry treatment without using the primer composition, thereby forming the adhesive layer 30 on the surface 12a. (FIG. 1 (c)).
  • the 2nd member 20 is bonded together on the adhesive bond layer 30 in a bonding process.
  • the laminated member 100 which has the 1st member 12, the contact bonding layer 32 (layer which the adhesive bond layer 30 hardened
  • the surface treatment step is a step of performing a dry treatment on the surface of the first member containing the crystalline thermoplastic resin so as to satisfy the condition A described later.
  • the first member used in the surface treatment step is not particularly limited as long as it is a member (preferably a base material) containing a crystalline thermoplastic resin.
  • the first member is preferably used as an inner member (inner member).
  • the crystalline thermoplastic resin is not particularly limited as long as it is a crystalline thermoplastic resin.
  • Specific examples thereof include polyolefin resins such as polyethylene, polypropylene, and polybutylene; methacrylic resins such as polymethyl methacrylate; polystyrene, ABS, Polystyrene resins such as AS; polyester resins such as polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate, polyethylene naphthalate (PEN), poly 1,4-cyclohexyldimethylene terephthalate (PCT); Polycaproamide (nylon 6), polyhexamethylene adipamide (nylon 66), polyhexamethylene sebamide (nylon 610), polyhexamethylene dodecamide (nylon 612), polydo Canamide (nylon 12), polyhexamethylene terephthalamide (nylon 6T), polyhexanemethylene isophthalamide (nylon 6I),
  • the content of the crystalline thermoplastic resin in the first member is preferably 10 to 100% by mass, and more preferably 60 to 100% by mass.
  • the first member is preferably a composite member containing a crystalline thermoplastic resin and an inorganic substance.
  • inorganic substances include silica, titanium oxide, magnesium oxide, antimony oxide, aluminum hydroxide, magnesium hydroxide, calcium hydroxide, calcium carbonate, talc, clay, mica, glass fiber, carbon black, graphite, and carbon fiber. Can be mentioned.
  • the first member may contain two or more inorganic substances.
  • the thickness is not particularly limited, but is preferably 1 ⁇ m to 100 mm.
  • a dry process will not be restrict
  • the dry treatment may be performed on the entire surface of the first member, or may be performed on a part of the surface of the first member. When the first member is a base material, it is preferably performed on one surface of the base material.
  • the dry treatment of the first member is a flame treatment, and a flame of reducing flame is applied to the surface of the first member in the flame treatment.
  • the dry process consists of a single dry process (one pass) (for example, one sweep), but also a plurality of unit dry processes (a plurality of passes) (for example, a plurality of sweeps). It doesn't matter.
  • the dry treatment consists of multiple unit dry treatments, even if the next unit dry treatment is performed without any interval (continuous treatment), the next unit dry treatment is performed after the member is allowed to cool after the unit dry treatment. It can be done (intermittent processing).
  • the flame treatment is a method of performing surface treatment with a flame (also referred to as flame or flame).
  • a flame also referred to as flame or flame.
  • a conventionally known method such as a method using a combustion apparatus such as a burner can be used.
  • the flame in the flame treatment means the entire flame ejected from the tip of the combustion device such as the burner.
  • the flame usually has an oxidation flame (outer flame) and a reducing flame (inner flame).
  • Oxidation flame refers to a portion outside the flame (region where oxygen supply is sufficient and fuel gas is completely burned). Oxidative flame is the hottest of all flames. (Reducing flame) The reducing flame refers to an inner portion of the flame than the oxidizing flame (region where oxygen supply is insufficient and fuel gas is incompletely burned). The reducing flame is cooler than the oxidizing flame.
  • the total length of the flame (the length from the tip of the combustion device to the tip of the flame) that can be used in the surface treatment process (for example, experimentally or industrially) is 20 to 300 mm from the viewpoint of excellent workability. Is preferable, and it is more preferable that it is 50 mm or more.
  • the length of the reducing flame (the length from the tip of the combustion device to the tip of the reducing flame (inner flame)) that can be used (for example, experimentally or industrially) in the surface treatment step can be, for example, 3 to 150 mm. From the viewpoint of excellent workability, it is preferably 5 mm or more.
  • the position of the surface of the substrate and the reducing flame is not particularly limited. It is only necessary that the surface of the substrate hits the reducing flame.
  • the position of the substrate can be a position between the tip of the combustion device (for example, a burner) and the tip of the reducing flame.
  • the position of the base material is excellent due to the effect of the present invention, and is reduced from the tip of the combustion device in the reducing flame from the viewpoint of excellent workability in consideration of the blur (fluctuation) range of the flame (flame) during the dry processing operation.
  • the middle part between the flame tips is preferred.
  • the distance between the tip of the combustion apparatus and the base material can be, for example, 3 to 150 mm, which is excellent due to the effects of the present invention.
  • the thickness is preferably 5 to 75 mm from the viewpoint of excellent workability in consideration of the shake (fluctuation) range.
  • the fuel gas used for the flame treatment examples include flammable gas (for example, propane gas, butane gas, city gas, natural gas, etc.), a mixed gas, or a combustion gas containing aerosol.
  • flammable gas for example, propane gas, butane gas, city gas, natural gas, etc.
  • mixed gas for example, propane gas, butane gas, city gas, natural gas, etc.
  • combustion gas containing aerosol for example, propane gas, butane gas, city gas, natural gas, etc.
  • the gas pressure in the flame treatment is preferably from 0.005 to 10 MPa, more preferably from 0.01 to 1.5 MPa, from the viewpoint that the effect of the present invention is excellent.
  • the frame processing speed is preferably 100 to 2,000 mm / sec, and more preferably 200 to 1,000 mm / sec.
  • the number of passes of frame processing is preferably 1 to 5 times, and more preferably 1 to 2 times.
  • the number of passes is preferably 1 to 2 from the viewpoint that the effect of the present invention is excellent, and that the hydrophilicity of the surface and / or excessive treatment on the surface is suppressed.
  • the shape of the tip of the combustion device (burner or the like) is not particularly limited. For example, a circle, an ellipse, a flat shape, a rectangle, and a square can be mentioned.
  • the inside of the shape is a cavity.
  • the inner diameter is preferably 5 to 30 mm.
  • the lateral width is preferably 5 to 500 mm, for example.
  • the vertical width can be set to 3 to 300 mm, for example.
  • the shape of the flame ejected from the tip of the combustion apparatus is not particularly limited.
  • rod shape, fan shape, and curtain shape are mentioned.
  • the wetness index of the surface of the first member obtained in the surface treatment step after the dry treatment is excellent due to the effects of the present invention, the surface is sufficiently hydrophilic and / or by the dry treatment on the surface. From the viewpoint that excessive treatment is suppressed, 34 to 60 dyn / cm is preferable, 38 to 58 dyn / cm is more preferable, and 40 to 50 dyn / cm is more preferable.
  • the wetting index was measured using a wetting reagent (Wako Pure Chemical Industries, Ltd.).
  • Step 2 Adhesive application step
  • an adhesive is applied to the surface of the first member that has been subjected to the dry treatment of the first member, and the adhesive is applied to the surface of the first member that has been subjected to the dry treatment. It is a process of forming a layer.
  • Adhesives are not particularly limited, but specific examples include acrylic adhesives, rubber adhesives, silicone adhesives, urethane adhesives, ⁇ -olefin adhesives, ether adhesives, ethylene-vinyl acetate.
  • Resin adhesive epoxy resin adhesive, vinyl chloride resin adhesive, chloroprene rubber adhesive, cyanoacrylate adhesive, aqueous polymer-isocyanate adhesive, styrene-butadiene rubber adhesive, nitrile rubber adhesive
  • Adhesives nitrocellulose adhesives, reactive hot melt adhesives, phenolic resin adhesives, modified silicone adhesives, polyamide resin adhesives, polyimide adhesives, polyurethane resin adhesives, polyolefin resin adhesives Agent, polyvinyl acetate resin adhesive, polystyrene resin solvent adhesive, polyvinyl alcohol Adhesive, polyvinylpyrrolidone resin adhesive, polyvinyl butyral resin adhesive, polybenzimidazole adhesive, polymethacrylate resin adhesive, melamine resin adhesive, urea resin adhesive, resorcinol adhesive, etc.
  • the urethane-based adhesive and the epoxy-based adhesive are preferably one-component type or two-component type.
  • the one-component urethane adhesive include a moisture curable adhesive containing a urethane prepolymer having an isocyanate group.
  • the two-pack type urethane adhesive include an adhesive containing a main agent containing a urethane prepolymer and a curing agent containing a polyol.
  • the one-pack type epoxy adhesive examples include room temperature curing or heat curing type adhesives including a latent curing agent such as ketimine, oxazolidine, aldimine compound and a liquid epoxy resin.
  • a latent curing agent such as ketimine, oxazolidine, aldimine compound and a liquid epoxy resin.
  • the two-pack type epoxy resin adhesive for example, a main agent selected from liquid epoxy resins (for example, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AD type epoxy resin, or novolac type epoxy resin) and the like .
  • An adhesive containing a curing agent for example, a chain aliphatic amine, a cyclic aliphatic amine or an aromatic amine, a nitrogen-containing aromatic amine curing agent such as an imidazole compound, an amidoamine curing agent, a ketimine). Is mentioned.
  • the method of applying the adhesive to the surface of the first member that has been dry-treated is not particularly limited.
  • the thickness of the formed adhesive layer is not particularly limited, but is preferably 0.1 to 20 mm.
  • Step 3 Bonding step
  • the bonding step is a step of bonding the second member onto the above-described adhesive layer.
  • a laminated member having the first member, the adhesive layer (the layer in which the adhesive layer is cured), and the second member in this order is obtained.
  • ⁇ Second member> The material in particular of the 2nd member is not restrict
  • resin the crystalline thermoplastic resin mentioned above is mentioned, for example.
  • the second member is preferably used as an outer member (outer member). From the viewpoint of further improving the adhesion between the second member and the adhesive layer, the surface of the second member may be subjected to coating or the above-described dry treatment before the second member is bonded.
  • a surface treatment step is further performed before the bonding step, in which a dry treatment is performed on the surface of the second member so as to satisfy the following condition A2. It is also preferable.
  • the surface of the second member subjected to the surface treatment is bonded onto the above-described adhesive layer.
  • the dry treatment of the second member is a flame treatment, and a flame of reducing flame is applied to the surface of the second member in the flame treatment.
  • the laminated member produced by the method of the present invention is excellent in adhesiveness, it is particularly useful for automobile interior and exterior members such as automobile bodies, front doors, rear doors, back doors, front bumpers, rear bumpers, and rocker moldings.
  • Each component of the following Table 1 was mixed with a composition (parts by mass) shown in the same table using a stirrer to prepare a main agent shown in the upper part of the table and a curing agent shown in the lower part of the table. Next, 100 g of the prepared main agent and 10 g of the curing agent were mixed to obtain adhesives 1 and 2.
  • the adhesive 1 is a urethane adhesive
  • the adhesive 2 is an epoxy adhesive.
  • Epoxy resin 1 Adeka Resin EP-4100 (manufactured by Adeka)
  • Epoxy resin 2 Adeka Resin EP-4006 (manufactured by Adeka)
  • Compound 1 Isocyanurate of hexamethylene diisocyanate (Tolonate HDT, manufactured by Perstorp) -Compound 2: Daimalon (manufactured by Yasuhara Chemical Co., Ltd.) ⁇ Carbon black: # 200MP (manufactured by Shin Nikka Carbon) ⁇ Calcium carbonate 1: Super S (Maruo Calcium) ⁇ Calcium carbonate 2: Calfine 200 (manufactured by Maruo Calcium) ⁇ Plasticizer 1: Diisononyl phthalate (J-PLUS) ⁇ Plasticizer 2: Shellsol TM (manufactured by Japan Chemtech) Catalyst 1: Dimorpholinodiethyl ether (manufactured by San Apro)
  • Base material made of polypropylene composite material (R-200G, manufactured by Prime Polymer Co., Ltd.) (polypropylene content: 80 mass%, inorganic substance (glass filler) content: 20 mass%) (width: 25 mm,
  • first member made of polypropylene composite material (R-200G, manufactured by Prime Polymer Co., Ltd.) (polypropylene content: 80 mass%, inorganic substance (glass filler) content: 20 mass%) (width: 25 mm,
  • frame represents frame processing.
  • “Oxidation flame” indicates that the flame was applied to the surface of the substrate.
  • Reducing flame indicates that the reducing flame was applied to the surface of the substrate in the flame treatment. Details of each frame processing will be described later. In Comparative Example 1, no dry treatment was performed.
  • Adhesive application process Next, the adhesive agent described in Table 2 was directly applied to the surface of the first member subjected to the dry treatment to form an adhesive layer (thickness: 3 mm). No primer composition was used in the adhesive application step.
  • CF numerical value indicates the ratio (%) of the area of cohesive failure
  • AF numerical value indicates the ratio (%) of the area of interfacial debonding.
  • CF90AF10 indicates that the area ratio of cohesive failure is 90% and the area ratio of interfacial debonding is 10%.
  • the ratio of the area of cohesive failure is preferably 90% or more, more preferably 95% or more, and further preferably 100%.
  • Example 9 to 12 gas pressure 2.0 MPa
  • the flame treatment was performed under the conditions shown in Table 2 using a burner having a circular tip and an inner diameter of 6 mm. Specifically, the burner (frame) was swept with respect to the base material by moving the burner with respect to the fixed base material.
  • LPG mixed propane and butane
  • the speed in Table 2 is the speed of the frame processing, specifically, the speed [mm / sec] at which the burner is moved with respect to the fixed base material.
  • the total length of the flame is the length [mm] from the tip of the burner to the tip of the flame (including the oxidation flame and the reduction flame).
  • the length of the reducing flame is the length [mm] from the tip of the burner to the tip of the reducing flame (inner flame).
  • the distance is the distance [mm] between the tip of the burner and the substrate.
  • the number of passes is the number of times the burner (frame) has been swept.
  • the burner is swept once from one end to the other end of the substrate, and when the number of passes is described as “2”, the burner is used as the substrate. The burner was swept once from one end to the other end, and then the burner was swept from the other end to the other end. What is described as “continuous” when the number of passes is two or more is the result of performing the next sweep without any interval (continuous processing).
  • the gas pressure is the pressure of the fuel gas used for flame processing.
  • “wetting index” represents the wetting index [dyn / cm] of the surface of the first member subjected to the dry treatment.
  • the wetting index was measured using a wetting reagent (manufactured by Wako Pure Chemical Industries, Ltd.). Evaluation Criteria In the present invention, when the wetting index is less than 34, it is considered that the surface of the member is not sufficiently hydrophilized. When the wetting index is 34 to 50 or less, it is considered that the excessive treatment by the dry treatment can be extremely suppressed, and the surface of the member is very appropriately hydrophilized and indicates that they are balanced.
  • wetting index is more than 50 and 64 or less, it is considered that the excessive treatment by the dry treatment can be somewhat suppressed or the surface of the member is slightly hydrophilized. If the wetting index exceeds 64, it is considered that the excessive treatment by the dry treatment could not be suppressed.
  • the laminated member obtained from the manufacturing method of the present example that was dry-treated so as to satisfy the specific conditions showed excellent adhesion without using a primer.
  • the number of passes was 2 or less, the adhesiveness was very excellent (Examples 1, 2, 5, 6, 9, 10, 13).
  • the wetting index is 34 to 64, excellent adhesiveness can be obtained.

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Abstract

本発明は、プライマーを使用しなくても優れた接着性を示す積層部材の製造方法を提供する。本発明は、結晶性熱可塑性樹脂を含有する第１部材と接着層と第２部材とをこの順に有する積層部材を製造する積層部材の製造方法であって、結晶性熱可塑性樹脂を含有する第１部材の表面に対して下記条件Ａを満たすように乾式処理を行う表面処理工程と、第１部材の乾式処理を行った表面にプライマー組成物を介さずに接着剤を付与して第１部材の乾式処理を行った表面に接着剤層を形成する接着剤付与工程と、接着剤層上に第２部材を貼り合わせる、貼り合わせ工程とを備える、積層部材の製造方法である。 （条件Ａ）第１部材の上記乾式処理が、フレーム処理であり、フレーム処理において火炎の還元炎を第１部材の表面に当てる。

Description

積層部材の製造方法
　本発明は、積層部材の製造方法に関する。
　従来、自動車のボディ、フロントドア、リヤドア、バックドア、フロントバンパー、リアバンパー、ロッカーモールなど自動車の内外装部材には、鋼板が使用されているが、自動車の軽量化を図る観点から、一部に、ポリプロピレン樹脂などの結晶性熱可塑性樹脂が使用されることが増えてきている。
　このように自動車の内外装部材に樹脂を使用する場合、通常、樹脂部材の接着面に対してプライマー組成物を塗布してから接着剤を塗布して貼り合わせることが行われている。
　また、プライマーを使用しなくても優れた接着性を示す積層部材の製造方法を提供することを目的として、結晶性熱可塑性樹脂を含有する第１部材と、接着層と、第２部材とをこの順に有する積層部材を製造する、積層部材の製造方法であって、結晶性熱可塑性樹脂を含有する第１部材の表面に対して、特定条件を満たすように乾式処理を行う、表面処理工程と、上記第１部材の上記乾式処理を行った表面に、プライマー組成物を介さずに、接着剤を付与して、上記第１部材の前記乾式処理を行った表面に接着剤層を形成する、接着剤付与工程と、上記接着剤層上に第２部材を貼り合わせる、貼り合わせ工程とを備える、積層部材の製造方法が提案されている（例えば、特許文献１）。
特開２０１７－１２８０５２号公報
　昨今、自動車に対して安全性や燃費などの要求水準が高まるなか、積層部材の接着性（接着させた部材同士の接着性）に対してもさらなる向上が求められている。
　このようななか、本発明者らが特許文献１を参考に、プライマーを使用せずに、乾式処理と接着剤を用いて積層部材を製造したところ、その接着性は必ずしも満足できるものではないことが明らかになった。
　そこで、本発明は、上記実情を鑑みて、プライマーを使用しなくても優れた接着性を示す積層部材の製造方法を提供することを目的とする。
　本発明者らは、上記課題について鋭意検討した結果、結晶性熱可塑性樹脂を含有する部材に対して特定の条件を満たすように乾式処理を行うことで、上記課題を解決できることを見出した。
　すなわち、本発明者らは、以下の構成により上記課題が解決できることを見出した。
［１］　結晶性熱可塑性樹脂を含有する第１部材と、接着層と、第２部材とをこの順に有する積層部材を製造する、積層部材の製造方法であって、
　結晶性熱可塑性樹脂を含有する第１部材の表面に対して、下記条件Ａを満たすように乾式処理を行う、表面処理工程と、
　上記第１部材の上記乾式処理を行った表面に、プライマー組成物を介さずに、接着剤を付与して、上記第１部材の上記乾式処理を行った表面に接着剤層を形成する、接着剤付与工程と、
　上記接着剤層上に第２部材を貼り合わせる、貼り合わせ工程とを備える、積層部材の製造方法。
（条件Ａ）上記第１部材の上記乾式処理が、フレーム処理であり、上記フレーム処理において火炎の還元炎を上記第１部材の表面に当てる。
［２］　上記第２部材が、塗装された部材である、［１］に記載の積層部材の製造方法。
［３］　上記第１部材が、上記結晶性熱可塑性樹脂であるポリオレフィン系樹脂と無機物とを含む複合素材である、［１］又は［２］に記載の積層部材の製造方法。
［４］　上記接着剤が、ウレタン系接着剤、エポキシ系接着剤、変性シリコーン系接着剤、及び、アクリル系接着剤からなる群より選択される少なくとも１種である、［１］～［３］のいずれかに記載の積層部材の製造方法。
［５］　上記第２部材が、結晶性熱可塑性樹脂を含有し、
　上記貼り合わせ工程の前に、さらに、上記第２部材の表面に対して、下記条件Ａ２を満たすように乾式処理を行う、表面処理工程を備え、
　上記貼り合わせ工程において、上記接着剤層上に、上記第２部材の上記表面処理を行った側の表面を貼り合わせる、［１］～［４］のいずれかに記載の積層部材の製造方法。
（条件Ａ２）上記第２部材の上記乾式処理が、フレーム処理であり、上記フレーム処理において火炎の還元炎を上記第２部材の表面に当てる。
　以下に示すように、本発明によれば、プライマーを使用しなくても優れた接着性を示す積層部材の製造方法を提供することができる。
図１は、本発明の製造方法の一実施態様を工程順に示す模式的断面図である。
　以下に、本発明の積層部材の製造方法について説明する。
　なお、本明細書において「～」を用いて表される数値範囲は、「～」の前後に記載される数値を下限値および上限値として含む範囲を意味する。
　本発明の積層部材の製造方法（以下、単に「本発明の方法」とも言う）は、結晶性熱可塑性樹脂を含有する第１部材と、接着層と、第２部材とをこの順に有する積層部材を製造する、積層部材の製造方法であって、下記３つの工程を備える。
（１）工程１：表面処理工程
　結晶性熱可塑性樹脂を含有する第１部材の表面に対して、後述する条件Ａを満たすように乾式処理を行う工程
（２）工程２：接着剤付与工程
　上記第１部材の上記乾式処理を行った表面に、プライマー組成物を介さずに、接着剤を付与して、上記第１部材の上記乾式処理を行った表面に接着剤層を形成する工程
（３）工程３：貼り合わせ工程
　上記接着剤層上に第２部材を貼り合わせる工程
　本発明の方法はこのような構成をとるため、得られる積層体は優れた密着性を示すものと推測される。その理由は明らかではないが、およそ以下のとおりと推測される。
　本発明では、結晶性熱可塑性樹脂を含有する部材の表面に対して後述する条件Ａ（以下、条件Ａを「特定条件」とも言う）を満たすように乾式処理するため、上記乾式処理において上記表面に火炎の酸化炎（外炎）を当てる場合よりも、条件がマイルドであり、乾式処理による過剰処理を抑制することができ、部材の最表面の結晶性が崩れることなく、部材の表面が親水化されると考えられる。そのため、親水化された部材の表面に接着剤が馴染んで表面全体に十分に密着した接着剤層が形成されるとともに、接着剤層から形成された接着層は、部材の最表面の結晶構造がアンカーとなって部材に強く固定されるものと考えられる。結果として、プライマー組成物を使用しなくても優れた接着性を示す積層部材が得られるものと考えられる。
　まず、図面を用いて、本発明の製造方法について説明する。
　図１は、本発明の製造方法の一実施態様を工程順に示す模式的断面図である。
　図１（ａ）は、表面処理工程で使用される第１部材１０を表す。
　まず、表面処理工程において、第１部材１０の表面１０ａに対して特定条件を満たすように乾式処理を行う。このようにして、乾式処理後の第１部材１２が得られる（図１（ｂ））。
　次に、接着剤付与工程において、乾式処理後の第１部材１２の乾式処理を行った表面１２ａにプライマー組成物を介さずに接着剤を付与して、表面１２ａに接着剤層３０を形成する（図１（ｃ））。
　さらに、貼り合わせ工程において、接着剤層３０上に第２部材２０を貼り合わせる。このようして、第１部材１２と、接着層３２（接着剤層３０が硬化した層）と、第２部材２０とをこの順に有する積層部材１００が得られる（図１（ｄ））。
　以下、各工程について詳述する。
［工程１：表面処理工程］
　表面処理工程は、結晶性熱可塑性樹脂を含有する第１部材の表面に対して、後述する条件Ａを満たすように乾式処理を行う工程である。
＜第１部材＞
　表面処理工程で使用される第１部材は結晶性熱可塑性樹脂を含有する部材（好ましくは、基材）であれば特に制限されない。なお、本発明の方法により製造される積層部材が自動車のバックドアなど、自動車用外装部材として用いられる場合、第１部材は内側の部材（インナー部材）として用いられるのが好ましい。
　結晶性熱可塑性樹脂は結晶性の熱可塑性樹脂であれば特に制限されず、その具体例としては、ポリエチレン、ポリプロピレン、ポリブチレンなどのポリオレフィン系樹脂；ポリメチルメタクリレートなどのメタクリル系樹脂；ポリスチレン、ＡＢＳ、ＡＳなどのポリスチレン系樹脂；ポリエチレンテレフタレート（ＰＥＴ）、ポリブチレンテレフタレート（ＰＢＴ）、ポリトリメチレンテレフタレート、ポリエチレンナフタレート（ＰＥＮ）、ポリ１，４－シクロヘキシルジメチレンテレフタレート（ＰＣＴ）などのポリエステル系樹脂；ポリカプロアミド（ナイロン６）、ポリヘキサメチレンアジパミド（ナイロン６６）、ポリヘキサメチレンセバカミド（ナイロン６１０）、ポリヘキサメチレンドデカミド（ナイロン６１２）、ポリドデカンアミド（ナイロン１２）、ポリヘキサメチレンテレフタラミド（ナイロン６Ｔ）、ポリヘキサンメチレンイソフタラミド（ナイロン６Ｉ）、ポリカプロアミド／ポリヘキサメチレンテレフタルアミドコポリマー（ナイロン６／６Ｔ）、ポリヘキサメチレンアジパミド／ポリヘキサメチレンテレフタルアミドコポリマー（ナイロン６６／６Ｔ）、ポリヘキサメチレンアジパミド／ポリヘキサメチレンイソフタルアミドコポリマー（ナイロン６６／６Ｉ）などのナイロン樹脂およびナイロン共重合体樹脂から選ばれるポリアミド樹脂；ポリ塩化ビニル樹脂；ポリオキシメチレン（ＰＯＭ）；ポリカーボネート（ＰＣ）樹脂；ポリフェニレンサルファイド（ＰＰＳ）樹脂；変性ポリフェニレンエーテル（ＰＰＥ）樹脂；ポリエーテルイミド（ＰＥＩ）樹脂；ポリスルホン（ＰＳＦ）樹脂；ポリエーテルスルホン（ＰＥＳ）樹脂；ポリケトン樹脂；ポリエーテルニトリル（ＰＥＮ）樹脂；ポリエーテルケトン（ＰＥＫ）樹脂；ポリエーテルエーテルケトン（ＰＥＥＫ）樹脂；ポリエーテルケトンケトン（ＰＥＫＫ）樹脂；ポリイミド（ＰＩ）樹脂；ポリアミドイミド（ＰＡＩ）樹脂；フッ素樹脂；これらの樹脂を変性させた変性樹脂またはこれらの樹脂の混合物などが挙げられる。なかでも、ポリオレフィン系樹脂であることが好ましく、ポリエチレン、ポリプロピレンがより好ましく、ポリプロピレンがさらに好ましい。第１部材は、２種以上の結晶性熱可塑性樹脂を含有していてもよい。
　第１部材中の結晶性熱可塑性樹脂の含有量は、１０～１００質量％であることが好ましく、６０～１００質量％であることがより好ましい。
　第１部材は、結晶性熱可塑性樹脂及び無機物を含有する複合部材であることが好ましい。無機物としては、例えば、シリカ、酸化チタン、酸化マグネシウム、酸化アンチモン、水酸化アルミニウム、水酸化マグネシウム、水酸化カルシウム、炭酸カルシウム、タルク、クレー、マイカ、ガラス繊維、カーボンブラック、グラファイト、カーボン繊維などが挙げられる。第１部材は、２種以上の無機物を含有していてもよい。
　第１部材が基材（平板状）である場合、その厚みは特に制限されないが、１μｍ～１００ｍｍであることが好ましい。
＜乾式処理＞
　乾式処理は、後述する条件Ａ（特定条件）を満たす乾式処理であれば特に制限されない。乾式処理は第１部材の表面の全体に行ってもよいし、第１部材の表面の一部に行ってもよい。第１部材が基材である場合、基材の一方の表面に行うのが好ましい。
（条件Ａ）上記第１部材の上記乾式処理が、フレーム処理であり、上記フレーム処理において火炎の還元炎を上記第１部材の表面に当てる。
　乾式処理は、１回の乾式処理（１回のパス）（例えば、１回の掃引）からなるのでも、複数回の単位乾式処理（複数回のパス）（例えば、複数回の掃引）からなるのでも構わない。乾式処理が複数回の単位乾式処理からなる場合、間隔を空けずに次の単位乾式処理を行っても（連続処理）、単位乾式処理後に部材の放冷を行ってから次の単位乾式処理を行っても（間欠処理）構わない。
＜＜フレーム処理＞＞
　フレーム処理は、フレーム（炎又は火炎とも言う。）によって表面処理する方法である。
　フレーム処理は、例えば、バーナーのような燃焼装置を用いる方法など、従来公知の方法を用いることができる。
＜火炎＞
　本発明において、フレーム処理における火炎は、上記バーナー等の燃焼装置の先端から噴出する炎全体を意味する。
　火炎は、通常、酸化炎（外炎）と還元炎（内炎）とを有する。
（酸化炎）
　上記酸化炎は、火炎の外側の部分（酸素供給が十分であり、燃料ガスが完全燃焼する領域）をいう。酸化炎は火炎全体の中で最も高温である。
（還元炎）
　上記還元炎は、火炎において上記酸化炎よりも内側の部分（酸素供給が不十分であり、燃料ガスが不完全燃焼する領域）をいう。還元炎は酸化炎よりも低温である。
（火炎の長さ）
　表面処理工程において（例えば実験あるいは工業的に）使用されうる火炎全体の長さ（燃焼装置の先端から火炎の先端までの長さ）は、作業性に優れるという観点から、２０～３００ｍｍであることが好ましく、５０ｍｍ以上であることがより好ましい。
（還元炎の長さ）
　表面処理工程において（例えば実験あるいは工業的に）使用されうる還元炎の長さ（燃焼装置の先端から還元炎（内炎）の先端までの長さ）は、例えば３～１５０ｍｍとすることができ、作業性に優れるという観点から５ｍｍ以上であることが好ましい。
（基材の表面と還元炎との位置）
　本発明において、基材の表面と還元炎との位置については特に制限されない。基材の表面が還元炎に当たればよい。基材の位置は、燃焼装置（例えばバーナー）の先端から還元炎の先端までの間の位置とできる。
　基材の位置は、本発明の効果により優れ、上記乾式処理作業時の炎（火炎）のブレ（揺らぎ）範囲を考慮した作業性に優れるという観点から、還元炎における、燃焼装置の先端から還元炎の先端までの間の中央部が好ましい。
（燃焼装置の先端と基材との距離）
　燃焼装置の先端と基材との距離（以下これを単に「距離」と称する場合がある）は、例えば３～１５０ｍｍとすることができ、本発明の効果により優れ、上記乾式処理作業時の炎のブレ（揺らぎ）範囲を考慮した作業性に優れるという観点から、５～７５ｍｍであることが好ましい。
（燃料ガス）
　フレーム処理に使用される燃料ガスとしては、例えば、引火性ガス（例えば、プロパンガス、ブタンガス、都市ガス、天然ガス等）、混合ガス又はエアゾールを含む燃焼ガスが挙げられる。
（ガス圧）
　フレーム処理におけるガス圧は、本発明の効果により優れるという観点から、０．００５～１０ＭＰａであることが好ましく、０．０１～１．５ＭＰａであることがより好ましい。
（フレーム処理の速度）
　フレーム処理の速度は、１００～２，０００ｍｍ／秒であることが好ましく、２００～１，０００ｍｍ／秒であることがより好ましい。
（フレーム処理のパス回数）
　フレーム処理のパス回数は、１～５回であることが好ましく、１～２回であることがより好ましい。
　上記パス回数は、本発明の効果により優れ、上記表面の親水化及び／又は上記表面に対する過剰処理が抑制されているという観点から、１～２回が好ましい。
（燃焼装置の先端の形状）
　燃焼装置（バーナー等）の先端の形状は特に制限されない。例えば、円形、楕円形、偏平形、長方形、正方形が挙げられる。なお上記形状の内部は空洞である。
　燃焼装置の先端が円形である場合、その内径は、５～３０ｍｍであることが好ましい。
　燃焼装置の先端が円形以外である場合、その横幅は例えば５～５００ｍｍであることが好ましい。また、その縦幅を例えば３～３００ｍｍとできる。
（火炎の形状）
　燃焼装置の先端から噴出する火炎の形状も特に制限されない。例えば、棒状、扇状、カーテン状が挙げられる。
（濡れ指数）
　上記表面処理工程で得られた第１部材の上記乾式処理を行った表面の濡れ指数は、本発明の効果により優れ、上記表面の親水化が十分である及び／又は上記表面に対する上記乾式処理による過剰処理が抑制されているという観点から、３４～６０ｄｙｎ／ｃｍが好ましく、３８～５８ｄｙｎ／ｃｍがより好ましく、４０～５０ｄｙｎ／ｃｍがより好ましい。
　本発明において、濡れ指数は、濡れ試薬（和光純薬社製）を使用して測定された。
［工程２：接着剤付与工程］
　接着剤付与工程は、上述した第１部材の乾式処理を行った表面に、プライマー組成物を介さずに、接着剤を付与して、上述した第１部材の乾式処理を行った表面に接着剤層を形成する工程である。
＜接着剤＞
　接着剤は特に限定されないが、その具体例としては、アクリル系接着剤、ゴム系接着剤、シリコーン系接着剤、ウレタン系接着剤、α－オレフィン系接着剤、エーテル系接着剤、エチレン－酢酸ビニル樹脂系接着剤、エポキシ樹脂系接着剤、塩化ビニル樹脂系接着剤、クロロプレンゴム系接着剤、シアノアクリレート系接着剤、水性高分子－イソシアネート系接着剤、スチレン－ブタジエンゴム系接着剤、ニトリルゴム系接着剤、ニトロセルロース系接着剤、反応性ホットメルト系接着剤、フェノール樹脂系接着剤、変性シリコーン系接着剤、ポリアミド樹脂系接着剤、ポリイミド系接着剤、ポリウレタン樹脂系接着剤、ポリオレフィン樹脂系接着剤、ポリ酢酸ビニル樹脂系接着剤、ポリスチレン樹脂溶剤系接着剤、ポリビニルアルコール系接着剤、ポリビニルピロリドン樹脂系接着剤、ポリビニルブチラール樹脂系接着剤、ポリベンズイミダソール系接着剤、ポリメタクリレート樹脂系接着剤、メラミン樹脂系接着剤、ユリア樹脂系接着剤、レゾルシノール系接着剤などが挙げられ、ウレタン系接着剤、エポキシ系接着剤、変性シリコーン系接着剤、及び、アクリル系接着剤からなる群より選択される少なくとも１種であるのが好ましく、ウレタン系接着剤であるのがより好ましい。
　ウレタン系接着剤及びエポキシ系接着剤は１液型または２液型であるのが好ましい。
　１液型ウレタン系接着剤としては、例えばイソシアネート基を有するウレタンプレポリマーを含む湿気硬化型接着剤が挙げられる。
　２液型ウレタン系接着剤としては、例えば、ウレタンプレポリマーを含む主剤と、ポリオールを含む硬化剤とを含有する接着剤が挙げられる。
　１液型エポキシ系接着剤としては、例えばケチミンやオキサゾリジン、アルジミン系化合物などの潜在性硬化剤と液状エポキシ樹脂を含む常温硬化または加熱硬化型接着剤が挙げられる。
　２液型のエポキシ樹脂系接着剤としては、例えば、液状エポキシ樹脂から選ばれる主剤（例えば、ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂、ビスフェノールＡＤ型エポキシ樹脂、又はノボラック型エポキシ樹脂等）と、硬化剤（例えば、鎖状脂肪族アミン、環状脂肪族アミンもしくは芳香族アミン等、イミダゾール化合物等の含窒素芳香族等のアミン系硬化剤、アミドアミン硬化剤、ケチミン等）とを含有する接着剤が挙げられる。
＜付与方法＞
　第１部材の乾式処理を行った表面に接着剤を付与する方法は特に限定されないが、例えば、ディップコーティング法、ダブルロールコータ、スリットコータ、エアナイフコータ、ワイヤーバーコータ、スライドホッパー、スプレーコーチィング、ブレードコータ、ドクターコータ、スクイズコータ、リバースロールコータ、トランスファーロールコータ、エクストロージョンコータ、カーテンコータ、ディップコーター、ダイコータ、グラビアロールによる塗工法、スクリーン印刷法、ディップコーティング法、スプレー塗布法、スピンコーティング法、インクジェット法などが挙げられる。
　形成される接着剤層の厚みは特に制限されないが、０．１～２０ｍｍであることが好ましい。
［工程３：貼り合わせ工程］
　貼り合わせ工程は、上述した接着剤層上に第２部材を貼り合わせる工程である。
　このようにして、第１部材と接着層（接着剤層が硬化した層）と第２部材とをこの順に有する積層部材が得られる。
＜第２部材＞
　第２部材の材料は特に制限されず、樹脂、ガラス、金属などが挙げられる。樹脂としては、例えば、上述した結晶性熱可塑性樹脂が挙げられる。
　なお、本発明の方法により製造される積層部材が自動車のバックドアなど、自動車用外装部材として用いられる場合、第２部材は外側の部材（アウター部材）として用いられるのが好ましい。
　第２部材と接着層との接着性をより向上させる観点から、第２部材を貼り合わせる前に、第２部材の表面に対して塗装や上述した乾式処理を行ってもよい。
＜貼り合わせ方法＞
　接着剤層上に第２部材を貼り合わせる方法は特に制限されないが、例えば、圧着する方法などが挙げられる。なお、接着剤を硬化させるために、第２部材を貼り合わせた後に、加熱処理等を行ってもよい。
　第２部材が結晶性熱可塑性樹脂を含有する場合、上記貼り合わせ工程の前に、さらに、第２部材の表面に対して、下記条件Ａ２を満たすように乾式処理を行う、表面処理工程を備えるのも好ましい。なお、貼り合わせ工程では、上述した接着層上に、第２部材の表面処理を行った側の表面を貼り合せる。
（条件Ａ２）上記第２部材の上記乾式処理が、フレーム処理であり、上記フレーム処理において火炎の還元炎を上記第２部材の表面に当てる。
　表面処理工程の具体例及び好適な態様は、上述した工程１と同じである。
［用途］
　本発明の方法によって製造される積層部材は接着性に優れるため、自動車のボディ、フロントドア、リヤドア、バックドア、フロントバンパー、リアバンパー、ロッカーモールなど自動車の内外装部材に特に有用である。
　以下、実施例により、本発明についてさらに詳細に説明するが、本発明はこれらに限定されるものではない。
＜接着剤の調製＞
　下記表１の各成分を、同表に示す組成（質量部）で撹拌機を用いて混合し、同表上段に示す主剤と同表下段に示す硬化剤とを調製した。
　次いで、調製した主剤１００ｇと、硬化剤１０ｇとを混合し、接着剤１～２を得た。
　上記接着剤１はウレタン系接着剤であり、上記接着剤２はエポキシ系接着剤である。
Figure JPOXMLDOC01-appb-T000001
　表１中の各成分の詳細は以下のとおりである。
（主剤）
・ポリマー１：下記で合成したウレタンプレポリマー
　ポリオキシプロピレンジオール（平均分子量２０００）７００ｇ、ポリオキシプロピレントリオール（平均分子量３０００）３００ｇ、および４，４′－ジイソシアネートフェニルメタン（分子量２５０）４９９ｇを混合し（この時ＮＣＯ／ＯＨ＝２．０）、更にフタル酸ジイソノニル５００ｇを加えて、窒素気流中、８０℃で１２時間撹拌を行い、反応させて、イソシアネート基を２．１０％含有するウレタンプレポリマー（ポリマー１）を合成した。
・ポリマー２：カネカＭＳポリマーＳ２０３（カネカ社製）
・エポキシ樹脂１：アデカレジンＥＰ－４１００（アデカ社製）
・エポキシ樹脂２：アデカレジンＥＰ－４００６（アデカ社製）
・化合物１：ヘキサメチレンジイソシネートのイソシアヌレート体（Ｔｏｌｏｎａｔｅ　ＨＤＴ、パーストープ社製）
・化合物２：ダイマロン（ヤスハラケミカル社製）
・カーボンブラック：＃２００ＭＰ（新日化カーボン社製）
・炭酸カルシウム１：スーパーＳ（丸尾カルシウム社製）
・炭酸カルシウム２：カルファイン２００（丸尾カルシウム社製）
・可塑剤１：フタル酸ジイソノニル（ジェイプラス社製）
・可塑剤２：シェルゾールＴＭ（ジャパンケムテック社製）
・触媒１：ジモルホリノジエチルエーテル（サンアプロ社製）
（硬化剤）
・化合物３：３官能ポリプロピレンポリオール（エクセノール１０３０、旭硝子社製）
・化合物４：ポリブタジエンジオール（Ｐｏｌｙ　ｂｄ　Ｒ－４５ＨＴ、出光興産社製、水酸基価：０．８ｍｏｌ／ｋｇ）
・化合物５：ターピネオール（ヤスハラケミカル社製）
・化合物６：３－グリシドキシプロピルトリメトキシシラン　サイラエース　Ｓ－５１０（チッソ社製）
・化合物７：ビニルトリメトキシシラン　ＫＢＭ　１００３（信越化学工業社製）
・化合物８：ケチミン型潜在性硬化剤　エピキュア　Ｈ－３０（三菱化学社製）
・炭酸カルシウム２：カルファイン２００（丸尾カルシウム社製）
・触媒１：ジモルホリノジエチルエーテル（サンアプロ社製）
・触媒２：スズ系触媒　ネオスタンＵ－３０３（日東化成社製）
＜積層部材の製造＞
（表面処理工程）
　ポリプロピレン複合材料（Ｒ－２００Ｇ、プライムポリマー社製）からなる基材（第１部材）（ポリプロピレンの含有量：８０質量％、無機物（ガラスフィラー）の含有量：２０質量％）（幅：２５ｍｍ、長さ：１２０ｍｍ、厚み：３ｍｍ）の一方の表面に表２に記載の処理条件で乾式処理を行った。表２の「処理方法」中、「フレーム」がフレーム処理を表す。「酸化炎」がフレーム処理において酸化炎を上記基材の表面に当てたことを表す。「還元炎」がフレーム処理において還元炎を上記基材の表面に当てたことを表す。各フレーム処理の詳細は後述する。なお、比較例１では乾式処理を行わなかった。
（接着剤付与工程）
　次に、第１部材の乾式処理を行った表面に、直接表２に記載の接着剤を付与して、接着剤層を形成した（厚み：３ｍｍ）。接着剤付与工程においてプライマー組成物は使用しなかった。
（貼り合わせ工程）
　さらに、接着剤層上に、塗装した別の基材（材料：ポリプロピレン）（幅：２５ｍｍ、長さ：１２０ｍｍ、厚み：３ｍｍ）（第２部材）を貼り合わせて、圧着し、２３℃、相対湿度５０％の環境下に３日間放置した。このようにして、第１部材と接着層（接着剤層が硬化した層）と第２部材とを備える積層部材を得た。
＜接着性の評価＞
・耐水試験等
　上記のとおり得られた積層部材について、耐水試験（５０℃の水に２週間浸漬）、耐熱試験（大気中、９０℃の条件下に２週間置く）又は耐湿熱試験（５０℃、相対湿度９５％ＲＨの条件下に２週間置く）を行った。
・剥離試験
　上記耐水試験等の後に得られた積層部材の接着層にナイフで切れ込みを入れ、手で第１部材と第２部材とを剥離する剥離試験を行った。そして、剥離面を目視で確認し、剥離面のうち、凝集破壊（ＣＦ）の面積の割合、及び、界面剥離（ＡＦ）の面積の割合を調べた。結果を表２に示す（初期）。
・・評価基準
　ここで、「ＣＦ数値」が凝集破壊の面積の割合（％）を示し、「ＡＦ数値」が界面剥離の面積の割合（％）を示す。例えば、「ＣＦ９０ＡＦ１０」は、凝集破壊の面積の割合が９０％で界面剥離の面積の割合が１０％であることを示す。
　なお、凝集破壊の面積の割合が多いほど接着性に優れることを表す。実用上、凝集破壊の面積の割合が９０％以上であることが好ましく、９５％以上であることがより好ましく、１００％であることがさらに好ましい。
Figure JPOXMLDOC01-appb-T000002
＜処理条件＞
（フレーム処理）
　本実施例におけるフレーム処理の詳細は以下のとおりである。
・ガス圧が０．０４ＭＰａであるフレーム処理（実施例１～８、１３、比較例２～９）
　実施例１～８、１３、比較例２～９のフレーム処理（ガス圧０．０４ＭＰａ）では先端が扇型であり、その弧の幅が２５ｍｍであり、中心角が１３５°であるバーナーを使用し、表２に記載の条件（速度、火炎全体の長さ、還元炎の長さ、距離、パス回数。以下同様）でフレーム処理を行った。具体的には、固定した基材に対してバーナーを動かすことで、バーナー（フレーム）を基材に対して掃引した。
・ガス圧２．０ＭＰａのフレーム処理（実施例９～１２）
　実施例９～１２のフレーム処理（ガス圧２．０ＭＰａ）では先端が円形であり、その内径が６ｍｍであるバーナーを使用し、表２に記載の条件でフレーム処理を行った。具体的には、固定した基材に対してバーナーを動かすことで、バーナー（フレーム）を基材に対して掃引した。
・フレーム処理の燃料ガス
　フレーム処理の燃料ガスとしてＬＰＧ（プロパン、ブタン混合）ガスを使用した。
　ここで、表２における速度とは、フレーム処理の速度であり、具体的には、固定した基材に対してバーナーを動かした速度［ｍｍ／秒］である。また、火炎全体の長さとは、バーナーの先端から火炎（酸化炎及び還元炎を含む）の先端までの長さ［ｍｍ］である。還元炎の長さとは、バーナーの先端から還元炎（内炎）の先端までの長さ［ｍｍ］である。距離とは、バーナーの先端と基材との間の距離［ｍｍ］である。また、パス回数とは、バーナー（フレーム）を掃引した回数である。例えば、パス回数が「１」と記載されているものはバーナーを基材の一端から他端まで１回掃引したものであり、パス回数が「２」と記載されているものはバーナーを基材の一端から他端まで１回掃引した後にもう１回他端から一端までバーナーを掃引したものである。パス回数が２回以上のものについて「連続」と記載されているものは間隔を空けずに次の掃引を行ったもの（連続処理）である。ガス圧とは、フレーム処理に使用された燃料ガスの圧力である。
（濡れ指数）
　表２中、「濡れ指数」は、第１部材の乾式処理を行った表面の濡れ指数［ｄｙｎ／ｃｍ］を表す。濡れ指数は、濡れ試薬（和光純薬社製）を使用して測定した。
・評価基準
　本発明において、濡れ指数が３４未満である場合、部材の表面の親水化が不足していると考えられる。
　濡れ指数が３４～５０以下である場合、乾式処理による過剰処理を非常に抑制することができ、部材の表面が非常に適切に親水化され、これらがバランスしていることを示すと考えられる。
　濡れ指数が５０を超え６４以下である場合、乾式処理による過剰処理をやや抑制することができた、又は、部材の表面がやや適切に親水化されたことを示すと考えられる。
　濡れ指数が６４を超える場合、乾式処理による過剰処理を抑制することができなかったことを示すと考えられる。
　表２から分かるように、特定条件を満たすように乾式処理を行った本実施例の製造方法から得られる積層部材は、プライマーを使用しなくても優れた接着性を示した。
　パス回数が２回以下である場合、接着性が非常に優れた（実施例１、２、５、６、９、１０、１３）。
　本発明において、濡れ指数が３４～６４である場合、優れた接着性を得ることができた。
　一方、フレーム処理がない比較例１又は特定条件を満たさない乾式処理を行った比較例２～９の製造方法から得られる積層部材は接着性が不十分であった。
　１０、１２　第１部材
　１０ａ、１２ａ　第１部材の表面
　２０　第２部材
　３０　接着剤層
　３２　接着層
　１００　積層部材

Claims (5)

  1. 　結晶性熱可塑性樹脂を含有する第１部材と、接着層と、第２部材とをこの順に有する積層部材を製造する、積層部材の製造方法であって、
    　結晶性熱可塑性樹脂を含有する第１部材の表面に対して、下記条件Ａを満たすように乾式処理を行う、表面処理工程と、
    　前記第１部材の前記乾式処理を行った表面に、プライマー組成物を介さずに、接着剤を付与して、前記第１部材の前記乾式処理を行った表面に接着剤層を形成する、接着剤付与工程と、
    　前記接着剤層上に第２部材を貼り合わせる、貼り合わせ工程とを備える、積層部材の製造方法。
    （条件Ａ）前記第１部材の前記乾式処理が、フレーム処理であり、前記フレーム処理において火炎の還元炎を前記第１部材の表面に当てる。
  2. 　前記第２部材が、塗装された部材である、請求項１に記載の積層部材の製造方法。
  3. 　前記第１部材が、前記結晶性熱可塑性樹脂であるポリオレフィン系樹脂と無機物とを含む複合素材である、請求項１又は２に記載の積層部材の製造方法。
  4. 　前記接着剤が、ウレタン系接着剤、エポキシ系接着剤、変性シリコーン系接着剤、及び、アクリル系接着剤からなる群より選択される少なくとも１種である、請求項１～３のいずれか１項に記載の積層部材の製造方法。
  5. 　前記第２部材が、結晶性熱可塑性樹脂を含有し、
    　前記貼り合わせ工程の前に、さらに、前記第２部材の表面に対して、下記条件Ａ２を満たすように乾式処理を行う、表面処理工程を備え、
    　前記貼り合わせ工程において、前記接着剤層上に、前記第２部材の前記表面処理を行った側の表面を貼り合わせる、請求項１～４のいずれか１項に記載の積層部材の製造方法。
    （条件Ａ２）前記第２部材の前記乾式処理が、フレーム処理であり、前記フレーム処理において火炎の還元炎を前記第２部材の表面に当てる。
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